Process for the production of granules, and granules thus obtained

ABSTRACT

A method for making solid granules containing aromatic, nutritional, dietary or cosmetic substances, wherein a core consisting of excipients optionally combined with active substances is formed for use as a carrier, and the core is coated in three steps with at least one layer, with one layer being formed in each step, by (a) coating the core with active substances optionally combined with excipients, (b) drying the layer and (c) screening the coated core. The method is preferably used to make granules that contain plant extracts and essential oils and may be chewed, sucked, swallowed or dissolved.

FIELD OF THE INVENTION

The present invention has for its object an original manufacturingprocess for the production of granules whose size, color, solubility andactive principles can vary according to the required final product:biogranules, aromatic granules, microgranules, pollen pearls, bathproducts. The assembly of these products will be better explained in thefollowing:

So that the aromas of these products will be sufficiently present, it isnecessary to use essential oils which are very volatile.

BACKGROUND OF THE INVENTION

FR-A-2,705,571 relates to the combination of two natural products, onebeing taken systematically as the base and is in the greater proportion:it is a fatty oil of animal or vegetable origin, the other is anaromatic essential oil extracted from a plant: melaleuca alternifolia,which can be replaced or associated with another aromatic essential oilof equivalent biochemical composition or conventionally known for itssimilar therapeutic effects, particularly on localized dental disorders:gum abscesses or any other paradontopathies having infectious orinflammatory characteristics.

FR-A-2,702,654 provides a cosmetic product permitting combatting anddiminishing loose skin at the epidermis. It is constituted by an activemixture of essential oils incorporated in a vegetable oil. This productis particularly adapted to improve the texture of the skin.

These documents provide only liquid substances which are more difficultto store, preserve and use.

Moreover, in the present century in which poor lifestyle hygiene isoften connected to undesirable eating habits, it is necessary to ingestnatural and balanced products.

To do that, it is known to use vegetal extracts.

FR-A-2,662,078 has for its object a cosmetic composition. Thecomposition according to this invention contains the following firstmaterials: a mineral substance for external use called clay, which iswhite, yellow, red or green, according to its origin and the density ofthe metalloids or minerals that it contains, in a concentration of 70 to80%; vegetal components, present in the form of plant flour andessential oils from plants, in a concentration of 18 to 19.5%; animalorigin components, present in the form of homeopathic dilutions,so-called "opotherapies" (organo-therapy), in a concentration of 0.5 to2%; in the composition ready to use, 100% of the first materials thusrepresenting 46% of the final formula, 54% of added water; the vegetalcomponents are marine algae, red grapevine, buttercup, cabbage,horsetail, and meadowsweet, to which are added essential oils oflavender, thyme or rosemary.

The mixture of the essential oils and the vegetal extracts are not veryhomogeneous amalgams. Moreover, the very volatile natural oils have atendency to evaporate and the aroma to disappear.

FR-A-2,657,255 discloses obtaining new cosmetic products. These have theparticularity of containing active principles in polymers which arethemselves grafted on particles of silica.

WO-A-93/00991 relates to a process for the production of medicalsubstances in the form of granules having a high apparent density, bydepositing by pulverization a cladding on the particles with an inertcore, with the help of a coating and granulating device by means ofsuccessive steps, first the constitution of a fluidized bed of particlesof material with an inert core inside the treatment chamber of acladding and granulating device, by causing to circulate a gaseouscurrent between the rotating disc and the internal wall of saidtreatment chamber, then the constitution of the granules by means ofdepositing a medication on the particles of core material, cladding themby pulverization with a solution of medicament; the process beingcharacterized by the fact that, during constitution of the granules, theparticles clad by pulverization are first transported toward a dryingzone surrounding the treatment chamber, secondly transported throughsaid drying zone by a gas current and thirdly returned to the treatmentchamber. The process of recirculation operates continuously untilgranules are constructed having the desired load of medication.

SUMMARY OF THE INVENTION

Generally speaking, it can be said that the characteristics which renderthe granules of the present invention original, compared to othercladding techniques, are the following:

Firstly, the assembly of the components used, active or excipient,constitute itself the starting core.

Secondly, the granule is thus homogenized in its composition, from thecenter to the outside, no matter what the size.

Thirdly, in the case of soluble granules, the granule is soluble totally(including the starting core) and the solubility (speed and medium) is afunction of the components (quality and quantity) and of the excipients.

Fourthly, the granule permits integration and hence good conservation ofthe volatile components such as essential oils.

To this end, the present invention relates to a process for theproduction of solid granules adapted to provide products that can bechewed, sucked, swallowed or dissolved, containing aromatic substances,foodstuffs, dietetic substances, or substances for cosmetic use,characterized in that it consists:

in providing a core, serving as a support, constituted by excipientsassociated or not with active substances, the excipient or activeprinciple is a solution which can for example be alcoholic,hydroalcoholic or aqueous,

covering the core in three steps, with at least one layer, these threesteps being carried out for each successive layer, by:

a) cladding the core with active substances associated or not withexcipients,

b) drying the layer, and

c) screening the covered core.

This process is carried out under vacuum in at least one turbinerotating about an axis for cladding.

The axis of each rotating turbine is inclined at an angle of 45 to 60°relative to the horizontal.

The process is carried out at a temperature comprised between 18 and 25°C., except for drying which is carried out at a maximum of 45° C. in anoven.

It is carried out at a humidity less than 70%.

The granules, obtained by means of the above process, are characterizedby the fact that they are each constituted of a central portion, formingthe core, and a peripheral portion, forming one or several concentriclayers; each layer is constituted by a component in solution and by acomponent in the form of a micronized powder.

On the one hand, the component in solution constitutes a cementingsolution whose density is greater than that of water. On the other hand,the component, in the form of powder, constitutes a volumetricconstituent.

The constituent in solution has a density comprised between 1010 and1020 and a fluidity index comprised between 16 and 20.

DETAILED DESCRIPTION OF THE INVENTION

According to a first embodiment, the composition of the granules issubstantially:

69% micronized maltisorb,

3.5% sodium bicarbonate,

3.5% citric acid,

21% concentrated fluid extract of plants, and

3% essential oils.

According to a second embodiment, the composition of the granules issubstantially:

85% of a mixture of sodium bicarbonate and citrate,

10% of essential oils,

4% of emulgine, and

1% of luviskol.

No matter what the embodiment, the core has a diameter less than 0.01mm, constituted of maltisorb or of a mixture of sodium bicarbonate andsodium citrate.

According to a particular embodiment, the core has a diametersubstantially 2 mm constituted by pollen grains.

The present invention relates to a process for the production ofgranules of all shapes, sizes, etc.

The essence of the invention resides in the fact that this process ischaracterized by the fact that it consists in providing on the one handa core serving as a support, and on the other hand, covering said corewith at least one layer.

More precisely, the core is always constituted by excipients which canbe or not associated with active substances. Similarly, each layer,which covers said core or a preceding layer disposed subjacently, isalways formed from active substances which can be associated withexcipients.

It is thus easy to understand that each layer which is deposited, willthen be subjected to drying, and finally screening of the core coveredby the dried layer.

These three steps, cladding, drying and screening, are each time carriedout for each layer of product covering the core or a subjacent layer.

So that the granules will be formed in the most homogeneous way, thereis used a stainless steel turbine which turns about an axis, itselfinclined at an angle of 45 to 60° relative to the horizontal.

Moreover, the conditions within this turbine are very precise; thus, thetemperature is always comprised between 18 and 25° C. except for dryingduring which the granules are ovened at 45° C. Moreover, the humiditymust necessarily be lower than 70%, so as to avoid any amalgamation ofthe granules in a same turbine.

All the turbine production phase is carried out under an air flow of2,500 m³ per hour.

In fact, the granules which are provided by the process are thusconstituted in a very homogeneous way from a central portion, formingthe core, and a peripheral portion, formed by one or several concentriclayers deposited according to the process.

The process requires the presence of three components having precisecharacteristics.

First of all the core, according to one preferred embodiment, is solidand in crystalline form or in crystals, and its diameter is less than0.01 mm.

There is then an excipient or active principle component which is insolution, for example alcoholic, hydroalcoholic or aqueous, with adensity which is greater than that of water. This component constitutesthe binding solution.

Finally, there is also a component constituted also by an excipient oran active principle in the form of micronized powder. This lattercomponent constitutes the volumetric component.

In any event, there is always at least one active principle among thethree components.

The core and the volumetric component can be identical. The idealdensity of the binding solution for practice of the process is 1010 fora fluidity index comprised between 16 and 20. Nevertheless, there can bea density comprised between 1010 and 1020.

As the case may be during preparation of the granules, it will benecessary to bring the solutions to the best density, either byconcentration or by dilution, as a function of the characteristics ofthe substance and of its compatibility with the diluent.

The ratio between the binding solution of ideal density and thevolumetric component is variable as a function of the final size of theproduct desired and of the density of the binding solution. But thisremains fixed during all the duration of the production process.

According to a particular embodiment, the composition of the granules issubstantially:

69% micronized maltisorb,

3.5% sodium bicarbonate,

3.5% citric acid,

21% concentrated fluid plant extract, and

3% essential oils.

According to another embodiment, the composition of the granules issubstantially:

85% of a mixture of sodium bicarbonate and sodium citrate,

10% essential oils,

4% emulgine, and

1% luviskol.

According to another embodiment, the core may be constituted byagglomerated pollen grains and have a diameter of substantially twomillimeters.

The assembly of these characteristics, which have been set forth,permits obtaining a range of products variable as to form, as a functionof the manner of use. Thus, these granules can be used either bydissolving them or by chewing them or by swallowing them.

These three sets of figures are used, for example, for all instances ofthe ingestion of active substances. But there can be used granules whichdissolve when it is desired to provide a solution such as an extract, atea, a bath or an inhalation.

The different uses are of course due to the composition of the vegetalextracts and the essential oils which are used.

Among the substances that can be provided, there are biogranules oforigin from a crystallized and calibrated maltisorb core. The fluidextracts and essential oils are deposited by pulverization.

When the fluid extracts are distributed uniformly over all the granules,the mask becomes binding and is worked only with difficulty in theturbine. The moisture contained in the core is absorbed by the additionof a certain quantity of mixture, thereby permitting free rotation. Itsuffices thus to let turn for several minutes with aspiration, so astotally to eliminate the alcohol contained in the hydro-alcoholicextracts, for example. Drying and screening follow to separate thegranules of different sizes.

When the first layer is crystallized, a second layer is applied underthe same conditions. The operation is then repeated to deposit, forsuccessive layers, all of the aromatic principles. The quantity and form(solid or liquid) of the principle contained in each granule define themean weight of each granule.

Another product is produced by the production of microgranules. This isin fact only a repetition of the biogranules, but with a smaller size.They can contain or not essential oils. The percentage of the componentscan vary as a function of the characteristics of solubility and ofconcentration of the required active principles.

Another product is constituted by vitamin pearls. In this case, thestarting core is constituted by natural pollen grains which have alreadybeen set forth above.

After the calibration of granules two millimeters in size, the pollencores are placed in the turbine and the technique which deposits thelayers, as described above, is used.

Finally, the last product relates to bath products. In this case, thestarting core and the volumetric component are constituted by a mixtureof sodium bicarbonate and citric acid. The binding solution isconstituted by essential oils, emulgine, luviskol and the coloring.

The production of course is carried out as previously given.

What is claimed is:
 1. Process for the production of solid granules,containing substances selected from the group consisting of nutritional,pharmaceutical, and cosmetic substances, which comprises:providing asolid core consisting of at least one excipient optionally associatedwith active substances for use as a support, the excipient or activeprinciple being in solution, covering the core, in three steps, with atleast one layer, the three steps being carried out for each successivelayer, by: a) coating the core with active substances optionallyassociated with excipients, said coating being carried out under vacuumin at least one turbine rotating about an axis, b) drying the layer, andc) screening the core covered by the dried layer to obtain the solidgranules; said process being carried out at a humidity of less than 70%,and at a temperature comprised between 18 and 25° C., except for thedrying step which is carried out at a maximum temperature of 45° C. inan oven.
 2. Process according to claim 1, wherein the axis of eachrotating turbine is inclined at an angle of 45 to 60° relative to thehorizontal.
 3. Solid granules, obtained by the process according toclaim 1, wherein each granule comprises a central portion forming thecore, and a peripheral portion forming one or several concentric layers;each layer comprising a component in solution and a component in theform of micronized powder.
 4. Granules according to claim 3, wherein thecomponent in solution is a binding solution whose density is greaterthan water, and the component in the form of a powder is a volumetriccomponent.
 5. Granules according to claim 3, wherein the component insolution has a density ranging between 1010 and 1020 and a fluidityindex ranging between 16 and
 20. 6. Granules according to claim 3,wherein the composition of the granules is substantially:69% ofmicronized maltisorb, 3.5% of sodium bicarbonate, 3.5% of citric acid,21% of fluid concentrated plant extract and 3% of essential oils. 7.Granules according to claim 3, wherein the composition of the granulesis substantially:85% of a mixture of sodium bicarbonate and sodiumcitrate, 10% of essential oils, 4% of emulgine, and 1% of luviskol. 8.Granules according to claim 6, wherein the core has a diameter smallerthan 0.01 mm, constituted by maltisorb.
 9. Granules according to claim7, wherein the core has a diameter smaller than 0.01 mm, constituted bya mixture of sodium bicarbonate and sodium citrate.
 10. Granulesaccording to claim 3, wherein the core has a diameter of about 2 mmconstituted by pollen grains.